CN106448986A - Anisotropic nanocrystalline rare earth permanent magnet and preparation method therefor - Google Patents

Anisotropic nanocrystalline rare earth permanent magnet and preparation method therefor Download PDF

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CN106448986A
CN106448986A CN201610847457.5A CN201610847457A CN106448986A CN 106448986 A CN106448986 A CN 106448986A CN 201610847457 A CN201610847457 A CN 201610847457A CN 106448986 A CN106448986 A CN 106448986A
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graphene
permanent magnet
earth permanent
magnet
nanocrystalline
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CN106448986B (en
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刘颖
王仁全
李军
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Sichuan University
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Sichuan University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266—Moulding; Pressing

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

The invention discloses an anisotropic nanocrystalline rare earth permanent magnet. The anisotropic nanocrystalline rare earth permanent magnet consists of nanocrystalline with the chemical formula of RE<a>Fe<100-a-b-c>B<b>TM<c> and graphene/or graphene microchips, wherein the content of the graphene/or graphene microchips is 0.01-1wt%; in the chemical formula of RE<a>Fe<100-a-b-c>B<b>TM<c>, a is greater than or equal to 28 and less than or equal to 33; b is greater than or equal to 0.9 and less than or equal to 1.35; c is greater than or equal to 0.15 and less than or equal to 7; RE is at least one of Ce, Nd, Pr or Dy; and TM is at least one of Ga, Co, Cu, Nb, Al, Zr, V, Si or Ti. The invention also provides a preparation method for the anisotropic nanocrystalline rare earth permanent magnet. The shortcomings of relatively low magnet slip coefficient of the rare earth permanent magnet material RE-Fe-B, harsh conditions of a contact surface of magnetic powder, difficulty in plastic deformation and the like are overcome; and the magnetic performance of the rare earth permanent magnet material is further improved.

Description

A kind of anisotropy nanocrystalline rare-earth permanent magnet and preparation method thereof
Technical field
The invention belongs to rare-earth permanent-magnet material technical field and in particular to a kind of anisotropy nanocrystalline rare-earth permanent magnet and Its preparation method.
Background technology
Nd-Fe-B permanent magnet material has excellent comprehensive such as high remanent magnetization, high coercivity and high magnetic energy product Close hard magnetic property, be widely used in the fields such as electromechanics, information, communication and medical treatment.Nanocrystalline Nd-Fe-B permanent magnet is steady due to temperature Qualitative, fracture toughness is superior to traditional micron crystalline substance sintered magnet, is one of study hotspot of current RE permanent magnetic alloy material.Heat Pressure/thermal deformation technique is to prepare one of effective means of theoretical density anisotropy Nd-Fe-B magnet.Because Nd-Fe-B magnet is deposited In Anisotropy, that is, the Young's moduluss of a, b axle are much larger than the Young's moduluss of c-axis, Nd-Fe-B crystal under the effect of the pressure Rotated by crystal-plane slip, crystal grain, " crystallization of the dissolution and precipitation " mechanism realizes preferential growth, form c-axis knitting parallel to pressure direction Structure.But due to principal phase Nd in Nd-Fe-B magnet2Fe14B is tetragonal phase structure, and slip system number is less, thus plastic deformation is more tired Difficult.Prior art is mainly adjusted by alloying component to improve plastic history.Leonowicz etc. [Leonowicz M, Davies H A.Effect of Nd content on induced anisotropy in hot deformed Fe-Nd-B magnets[J].Mater.Lett.,1994,19(5):275-279] have studied rare earth Nd content to anisotropy rare earth permanent magnet The impact of body performance is it is indicated that improve the deformation process that content of rare earth can improve alloy.But it is distributed in the rare-earth phase of intergranular in a large number Belong to non-magnetic phase, there is dilution effect, reduce the performance of magnet.Brown etc. [Brown D N, Smith B, Ma B M, et al.The dependence of magnetic properties and hot workability of rare earth-iron-boride magnets upon composition[J].IEEE Trans.Magn.,2004,40(4): 2895-2897] have studied add Rare-Earth Ce, impact to hot procedure and magnet performance of Pr, Dy and metal Co, Ga it is indicated that The rare earth of high level or alloying element are conducive to deformation process, but unnecessary alloy is mainly distributed on crystal boundary and forms second Phase, is non-magnetic phase, therefore equally has and releases magnetic effect, reduces magnet performance.Additionally, in hot pressing thermal deformation process, existing Method can not overcome due to rapidly quenched magnetic powder interface directly contact, and frictional resistance is larger, and low melting point intergranular phase in thermal deformation process It is extruded the contact surface bringing and there is periodicity coarse grain, make the problem that magnet performance reduces.
Content of the invention
Present invention aims to the deficiencies in the prior art, provide a kind of anisotropy of interpolation Graphene nanocrystalline Rare-earth permanent magnet and preparation method thereof, to overcome rare-earth permanent magnet slip system number less, magnetic powder contact surface inclement condition, plasticity The defects such as deformation difficulty, improve the magnetic property of rare-earth permanent magnet material simultaneously further.
Anisotropy nanocrystalline rare-earth permanent magnet of the present invention, this nanocrystalline rare-earth permanent magnet by chemical formula is REaFe100-a-b-cBbTMcNanocrystalline with Graphene and/or graphene microchip composition, wherein Graphene and/or graphene microchip Content be 0.01wt%～1wt%, described chemical formula REaFe100-a-b-cBbTMcIn, 28≤a≤33,0.9≤b≤1.35, 0.15≤c≤7, RE be Ce, Nd, Pr, Dy at least one, TM be Ga, Co, Cu, Nb, Al, Zr, V, Si, Ti at least A kind of.
The preparation method of anisotropy nanocrystalline rare-earth permanent magnet of the present invention, processing step is as follows：
With REaFe100-a-b-cBbTMcMagnetic powder is raw material with Graphene or graphite microchip, the quality of Graphene or graphite microchip Percent is 0.01%～1%, REaFe100-a-b-cBbTMcThe mass percent of magnetic powder is 99%～99.99%, will REaFe100-a-b-cBbTMcMagnetic powder mix homogeneously with Graphene or graphite microchip obtain mix magnetic powder, will mix magnetic powder room temperature, 3～the 10min that colds pressing under 100MPa～700MPa pressure obtains isotropism nanocrystalline magnet, or 400 DEG C～750 DEG C of temperature, Under pressure 100MPa～700MPa, hot pressing 3～10min obtains isotropism nanocrystalline magnet；To cold pressing again or hot pressing gained respectively to Same sex nanocrystalline magnet carries out thermal deformation 2min～8min under 650 DEG C～850 DEG C of temperature, pressure 50MPa～250MPa, obtains Anisotropy nanocrystalline rare-earth permanent magnet.
In said method, the structure level number of described Graphene is 1～10 layer, and Graphene thickness is 0.8～20nm, and piece footpath is 50～1000nm.
In said method, the structure level number of described graphene microchip is 11～100 layers, and thickness is 20～200nm, and piece footpath is 50～1000nm.
In said method, described hot pressing, thermal deformation are to be carried out using sensing heating or discharge plasma sintering mode, adopt During sensing heating, hot pressing temperature is 555 DEG C～755 DEG C, hot pressing pressure is 155MPa～355MPa, and heat distortion temperature is 655 DEG C ～855 DEG C, thermal deformation pressure be 155MPa～255MPa；During using discharge plasma sintering, hot pressing temperature is 455 DEG C～655 DEG C, hot pressing pressure be 255MPa～755MPa, heat distortion temperature be 655 DEG C～755 DEG C, thermal deformation pressure be 55MPa～ 255MPa.
In said method, during thermal deformation control deflection be 65%～75%, thus the speed of thermal deformation be 0.1mm/s～ 0.5mm/s.
In said method, thermal deformation can adopt following several ways：
A. restrained deformation (see Fig. 5) in Free Transform (see Fig. 4) and mould：Magnetic powder is loaded in hot pressing die and is pressed into Fine and close base substrate, is placed in shown in Fig. 4 or carries out thermal deformation deformation in thermal deformation mould shown in Fig. 5, obtain anisotropy after the demoulding Nanocrystalline composite.
B. back of the body crimp (see Fig. 7)：Magnetic powder is loaded the base substrate being pressed into densification in hot pressing die (see Fig. 3), the demoulding After be placed in back of the body extruding deforming mould (see Fig. 7) and carry out carrying on the back crimp, the demoulding remove two ends inhomogeneous deformation area obtain each to Different in nature radial orientation magnet ring.
Plus copper sheathing deformation method c.：First raw material magnetic powder is cold-pressed into base in mould (see Fig. 3), is placed in piece footpath after moving back mould bigger In the thermal deformation mould being provided with copper sheathing in pressed compact piece footpath (see Fig. 6), then directly deform in thermal deformation mould, formation is received Rice anisotropic crystalline rare-earth permanent magnet.
In the method for the invention, raw material REaFe100-a-b-cBbTMcMagnetic powder can be bought by market, also can be by with lower section Prepared by method：
(1) according to chemical formula REaFe100-a-b-cBbTMcDispensing, in described chemical formula, 28≤a≤33,0.9≤b≤1.35, 0.15≤c≤7, RE is at least one in Ce, Nd, Pr, Dy element, and TM is Ga, Co, Cu, Nb, Al, Zr, V, Si, Ti element In at least one；
(2) raw material preparing step (1) carries out melting, is cast in water cooled copper mould, obtains RE after meltingaFe100-a-b- cBbTMc-Alloy cast ingot；
(3) carry out fast melt-quenching after alloy cast ingot being crushed and obtain REaFe100-a-b-cBbTMcRapidly quenched magnetic powder.
Compared with prior art, the invention has the advantages that：
1. the invention provides a kind of anisotropy nanocrystalline rare-earth permanent magnet containing Graphene or graphene microchip, rich The rich type of rare earth permanent-magnetic material.
2. because Graphene or graphene microchip have excellent electric conductivity, heat conductivity, lubricity and mechanical property etc. Feature, thus after containing a certain proportion of Graphene or graphene microchip, the microstructure of magnet is obviously improved, and crystallite dimension is more Little, pattern is more regular, and more preferably, comprehensive magnetic can have a distinct increment crystal grain orientation.
3. the preparation method of anisotropy nanocrystalline rare-earth permanent magnet of the present invention is with REaFe155-a-b-cBbTMcMagnetic powder with Graphene or graphite microchip are raw material, and Graphene or graphite microchip nano powder are evenly distributed on contact circle of rapidly quenched magnetic powder granule Face, because it has good greasy property so that mutually slip or the inhibition rotating greatly reduce between magnetic powder particle, Be conducive to magnet hot-pressing densification and thermal deformation orientation process, overcome rare earth permanent-magnetic material RE-Fe-B magnet slip coefficient Mesh is less, and the difficult defect of plastic deformation, thus prepare the more excellent nanocrystalline rare-earth permanent magnet of performance.
4. anisotropy nanocrystalline rare-earth permanent magnet of the present invention with the addition of Graphene in preparation process, and Graphene has Have excellent conduction, heat conductivility, during discharge plasma sintering, due to granule between graphene powder is distributed with, strengthen Intergranular electric conductivity, faster, reach the temperature required time shortens granule heating rate, meanwhile, Graphene good heat conduction Property makes heat transfer speed between granule further speed up, and it is also shorter, before deformation that magnet integrally reaches consistent temperature required time Required temperature retention time shortens further, thus suppressing grain growth, is conducive to the raising of magnetic property；Using induction heating mode When, mainly utilize the excellent heat conductivility of Graphene, shortening heating and temperature retention time, thus suppressing grain growth, being conducive to magnetic The raising of performance.
5. the Graphene that anisotropy nanocrystalline rare-earth permanent magnet of the present invention adds before being deformed after all the time with free State form exist, be not involved in crystalline phase constitute, its be distributed between magnetic powder particle can with inhibiting grain growth, and Graphene have excellent Mechanical property, the performances such as the comprcssive strength of magnet can be lifted.
Brief description
Fig. 1 be embodiment 1 be obtained the microstructure of anisotropy nanocrystalline rare-earth permanent magnet and energy spectrum analysiss (figure a and Heat distortion magnet microcosmic texture features figure under figure b different multiplying；Figure c is that Graphene is distributed shape appearance figure in intercrystalline；Figure d is figure c The energy spectral line scanning result figure of middle boxed area).
Fig. 2 is that the fracture apperance figure of the anisotropy nanocrystalline rare-earth permanent magnet that embodiment 2 is obtained (schemes a for being not added with stone The magnet of black alkene, figure b is the magnet adding 0.2wt% Graphene).
Fig. 3 is hot pressing schematic diagram.
Fig. 4 is free thermal deformation schematic diagram (before wherein figure a is deformation, after figure b is deformation).
Fig. 5 is thermal deformation schematic diagram in mould.
Fig. 6 is to add copper sheathing thermal deformation schematic diagram (before wherein figure a is deformation, after figure b is for deformation).
Fig. 7 is back of the body crimp schematic diagram.
In Fig. 4～Fig. 7,1- magnetic powder, 2- pressure head；3- die sleeve, 4- hot-pressed magnets, 5- heat distortion magnet, 6- copper sheathing, 7- positions Ring.
Specific embodiment
Below by embodiment to the anisotropy nanocrystalline rare-earth permanent magnet adding Graphene of the present invention and its system Preparation Method is described further.
Embodiment 1
(1) according to chemical formula Nd29.89Fe66.15Co5.93Ga0.64B0.92Dispensing, raw materials used is more than 99.5% for purity Rare earth neodymium, purity is 99.99% gallium, and purity is 99.9% cobalt, the pure iron that purity is more than 99.9%, and Boron contents are The ferro-boron of 19.3wt%；
(2) by the Nd having configured29.89Fe66.15Co5.93Ga0.64B0.92Alloy raw material puts into intermediate frequency furnace melting rapid hardening earthenware In crucible, reach 10 in vacuum-2During more than Pa, power transmission preheats, and treats that vacuum reaches 10 again-2Stop evacuation after more than Pa And it is filled with high-purity Ar, when Ar air pressure reaches -0.05MPa in stove, the power of smelting furnace is adjusted and carries out melting to monitor system, Stirring after raw material all melts carries out refine 3min, after refine, aluminium alloy is poured in water cooled copper mould, obtains Nd29.89Fe66.15Co5.93Ga0.64B0.92Alloy cast ingot；
(3) alloy cast ingot coarse crushing is become the granule that particle diameter is 5～10mm, the ingot casting after then crushing is placed in vacuum electric In water jacketed copper crucible in arc quick quenching furnace, open electric arc and melt, after ingot casting melts completely, melt is passed through rotation molybdenum wheel and (turns Speed be 35m/s, piece footpath 250mm) cooling obtain amorphous rapidly quenched magnetic powder Nd29.89Fe66.15Co5.93Ga0.64B0.92；
(4) 100 eye mesh screens will be crossed after further for rapidly quenched magnetic powder ball mill crushing, then weigh this magnetic powder of 10g and (add with Graphene Dosage see table respectively, Graphene parameter：The number of plies be 1～10 layer, Graphene thickness be 0.8～20nm, piece footpath be 50～ Put into ball milling 5min in vacuum planetary ball mill tank after 500nm) mixing to obtain mixing magnetic powder, take out mixing magnetic under Ar gas shielded Powder is simultaneously put in preprepared hot pressing die, using discharging plasma sintering equipment in 600 DEG C of temperature, under pressure 200MPa Hot pressing obtain within 3 minutes close to densification isotropic magnet, then by gained isotropic magnet in Free Transform mode (see figure 4), under 700 DEG C, pressure 150MPa, 2～4min is deformed with the rate of deformation of 0.18mm/s and (when Graphene addition is different, becomes Shape easy degree has difference), deflection is 70%, obtains the anisotropy nanocrystalline rare-earth permanent magnetism of different Graphene additions Body.
Comparative example 1
In addition to without Graphene, according to method same as Example 1, prepare Nd29.89Fe66.15Co5.93Ga0.64B0.92 Magnet.
Gained is not added with the magnetic property such as following table with the anisotropy nanocrystalline rare-earth permanent magnet of different Graphene additions：
The microstructure of gained anisotropy nanocrystalline rare-earth permanent magnet (0.2g Graphene) and energy spectrum analysiss such as Fig. 1 institute Show, can be seen that magnet from Fig. 1 a and Fig. 1 b and formed by ribbon crystal grain stacking, intergranular or bar interband are dispersed with Nd-rich phase (white)；Can see, flaky graphite alkene is distributed in ribbon intercrystalline from Fig. 1 c intergranular enlarged drawing, Fig. 1 d is corresponding power spectrum Analysis, is further characterized by above-mentioned observed result.Add 1% Graphene (0.1g) although under the conditions of magnet performance decline, mainly Belong to non-magnetic phase owing to substantial amounts of Graphene, dilute magnet performance, lead to remanent magnetism and coercivity to decline, thus maximum magnetic flux Energy product decreases；But, after adding more Graphene, magnet resistance in deformation process is obviously reduced, and shortens deformation time, Reduce rock deformation pressure, provide new thinking for later preparation bulk heat distortion magnet.
Embodiment 2
(1) according to chemical formula MM29.6Fe63.2Co6.0Ga0.6Al0.2B1.0(MM is mischmetal, mainly comprises Ce, Nd, Pr, Micro Dy) dispensing, in raw materials used MM Ce be 49.8wt%, Nd be 25wt%, Pr be 25wt%, Dy be 0.2wt%, purity Gallium for 99.99%, purity is 99.9% cobalt, and purity is 99.95% aluminum, the pure iron that purity is more than 99.9%, Boron contents Ferro-boron for 19.3wt%；
(2) by the MM having configured29.6Fe63.2Co6.0Ga0.6Al0.2B1.0Alloy raw material puts into intermediate frequency furnace melting rapid hardening earthenware In crucible, reach 10 in vacuum-2During more than Pa, power transmission preheats, and treats that vacuum reaches 10 again-2Stop evacuation after more than Pa And it is filled with high-purity Ar, when Ar air pressure reaches -0.05MPa in stove, the power of smelting furnace is adjusted and carries out melting to monitor system, Stirring after raw material all melts carries out refine 3min, after refine, aluminium alloy is poured in water cooled copper mould, obtains MM29.6Fe63.2Co6.0Ga0.6Al0.2B1.0Alloy cast ingot；
(3) alloy cast ingot coarse crushing is become the granule that particle diameter is 5～10mm, the ingot casting after then crushing is placed in vacuum electric In water jacketed copper crucible in arc quick quenching furnace, open electric arc and melt, after ingot casting melts completely, melt is passed through rotation molybdenum wheel and (turns Speed be 28m/s, piece footpath 250mm) cooling obtain nanocrystalline rapidly quenched magnetic powder MM29.6Fe63.2Co6.0Ga0.6Al0.2B1.0；
(4) 100 eye mesh screens will be crossed after further for rapidly quenched magnetic powder ball mill crushing, then weigh this magnetic powder of 10g and 0.02g graphite Alkene (Graphene parameter：The number of plies be 1～10 layer, Graphene thickness be 0.8～20nm, piece footpath be 50～500nm) mixing after put into Obtain after ball milling 5min in vacuum planetary ball mill tank mixing magnetic powder, take out mixing magnetic powder under Ar gas shielded and put into prior preparation In good hot pressing die, using sensing hot pressing thermal deformation equipment in 600 DEG C of temperature, hot pressing under pressure 200MPa is connect for 10 minutes Closely fine and close isotropic magnet, then by gained isotropic magnet with Free Transform mode (see Fig. 4), in 750 DEG C, pressure Under 100MPa, 4min, deflection 75% are deformed with the rate of deformation of 0.15mm/s, obtain adding the anisotropy nanometer of Graphene Brilliant rare-earth permanent magnet.
Comparative example 2
In addition to without Graphene, according to method same as Example 2, prepare MM29.6Fe63.2Co6.0Ga0.6Al0.2B1.0Magnet.
Gained be not added with and with the addition of Graphene anisotropy nanocrystalline rare-earth permanent magnet magnetic property such as following table：
Shown in prepared fracture apperance Fig. 2 of anisotropy nanocrystalline rare-earth permanent magnet, micro- before and after contrast interpolation Graphene It can be seen that being not added with the magnet coarse grains of Graphene, orientation is poor for the change seeing structure, and obtain after adding Graphene Magnet crystallite dimension is obviously reduced, and is orientated more regular, Hard Magnetic phase RE of this nanocrystalline rare-earth permanent magnet2Fe14The crystallite dimension of B It is less than or is at least less than in one direction 100nm (shown in corresponding Fig. 2 (b)), thus magnet performance is obviously improved.
Embodiment 3
(1) according to chemical formula Ce33Fe66.15Ga0.5B1.35Dispensing, the raw materials used cerium for purity more than 99.5%, 99.99% gallium, the pure iron that purity is more than 99.9%, Boron contents are the ferro-boron of 19.3wt%；
(2) by the Ce having configured33Fe66.15Ga0.5B1.35Alloy raw material is put in intermediate frequency furnace melting rapid hardening crucible, Vacuum reaches 10-2During more than Pa, power transmission preheats, and treats that vacuum reaches 10 again-2Stop evacuation after more than Pa and be filled with height Pure Ar, when the power of smelting furnace is adjusted when reaching -0.05MPa and carries out melting to monitor system by Ar air pressure in stove, treats raw material After all melting, stirring carries out refine 3min, after refine, aluminium alloy is poured in water cooled copper mould, respectively obtains Ce33Fe66.15Ga0.5B1.35Alloy cast ingot；
(3) alloy cast ingot coarse crushing is become the granule that particle diameter is 5～10mm, the ingot casting after then crushing is placed in vacuum electric In water jacketed copper crucible in arc quick quenching furnace, open electric arc and melt, after ingot casting melts completely, melt is passed through rotation molybdenum wheel and (turns Speed be 33m/s, piece footpath 250mm) cooling obtain amorphous rapidly quenched magnetic powder Ce33Fe66.15Ga0.5B1.35；
(4) 100 eye mesh screens will be crossed after further for rapidly quenched magnetic powder ball mill crushing, then weigh this magnetic powder of 10g and (add with Graphene Dosage see table respectively, Graphene parameter：The number of plies be 1～10 layer, Graphene thickness be 0.8～20nm, piece footpath be 50～ 1000nm) mixing obtains after putting into ball milling 5min in vacuum planetary ball mill tank mixing magnetic powder, takes out and mixed under Ar gas shielded Close magnetic powder simultaneously to put in preprepared hot pressing die, using discharging plasma sintering equipment (SPS) in 550 DEG C of temperature, pressure Under power 100MPa, hot pressing obtains the isotropic magnet close to densification for 5 minutes, then by gained isotropic magnet with Free Transform Mode (see Fig. 4), under 700 DEG C, pressure 100MPa, deforms 3～5min (Graphene addition with the rate of deformation of 0.15mm/s When different, deformation easy degree has difference), deflection is 65%, obtains the anisotropy nanometer of different Graphene additions Brilliant rare-earth permanent magnet.
Comparative example 3
In addition to without Graphene, according to method same as Example 3, prepare Ce33Fe66.15Ga0.5B1.35.
Gained is not added with the magnetic property such as following table with the anisotropy nanocrystalline rare-earth permanent magnet of different Graphene additions：
Embodiment 4
(1) according to chemical formula Nd29.8Fe68.6Ga0.4Ti0.15Si0.1B0.95, raw materials used dilute more than 99.5% for purity Native neodymium, purity is 99.99% gallium, and purity is 99.5% titanium, and purity is 99.5% silicon, and purity is pure more than 99.9% Ferrum, Boron contents are the ferro-boron of 19.3wt%；
(2) by the Nd having configured29.8Fe68.6Ga0.4Ti0.15Si0.1B0.95Alloy raw material puts into intermediate frequency furnace melting rapid hardening In crucible, reach 10 in vacuum-2During more than Pa, power transmission preheats, and treats that vacuum reaches 10 again-2Stop after more than Pa taking out very Sky is simultaneously filled with high-purity Ar, adjusts the power of smelting furnace when Ar air pressure reaches -0.05MPa in stove and is melted to monitor system Refining, stirring after raw material all melts carries out refine 3min, after refine, aluminium alloy is poured in water cooled copper mould, obtains Nd29.8Fe68.6Ga0.4Ti0.15Si0.1B0.95Alloy cast ingot；
(3) alloy cast ingot coarse crushing is become the granule that particle diameter is 5～10mm, the ingot casting after then crushing is placed in vacuum electric In water jacketed copper crucible in arc quick quenching furnace, open electric arc and melt, after ingot casting melts completely, melt is passed through rotation molybdenum wheel and (turns Speed be 28m/s, piece footpath 250mm) cooling obtain nanocrystalline rapidly quenched magnetic powder Nd29.8Fe68.6Ga0.4Ti0.15Si0.1B0.95；
(4) 100 eye mesh screens will be crossed after further for rapidly quenched magnetic powder ball mill crushing, then weigh this magnetic powder of 10g and 0.5g graphite Alkene (Graphene parameter：The number of plies is 1～10 layer, and Graphene thickness is 0.8～20nm, and piece footpath is 50～1000nm) mix and put into very In null celestial body grinding jar, ball milling 10min obtains mixing magnetic powder, takes out mixing magnetic powder putting into and be ready in advance under Ar gas shielded Hot pressing die in, using induction heater in 660 DEG C of temperature, under pressure 200MPa hot pressing obtain within 5 minutes each close to densification To same sex magnet, then by gained isotropic magnet in back of the body extrusion die (see Fig. 7), in 850 DEG C, pressure 150～250MPa Under (in the backward, resistance is bigger, and required extruding force is also bigger), 6min is deformed with the rate of deformation of 0.2mm/s, obtains external diameter 30, Internal diameter 24, the extrusion ring magnet of wall thickness 3mm.
Comparative example 4
In addition to without Graphene, according to method same as Example 4, prepare Nd29.8Fe68.6Ga0.4Ti0.15Si0.1B0.95Magnet.
Gained be not added with and with the addition of Graphene anisotropy nanocrystalline rare-earth permanent magnet magnetic property such as following table：
Embodiment 5
(1) according to chemical formula Ce28Fe66.22Nb0.1Cu0.05B1.08, the raw materials used cerium for purity more than 99.5%, purity Niobium for 99.6%, purity is 99.9% copper, the pure iron that purity is more than 99.9%, and Boron contents are the ferro-boron of 19.3wt%；
(2) by the Ce having configured28Fe66.22Nb0.1Cu0.05B1.08Alloy raw material puts into intermediate frequency furnace melting rapid hardening crucible Interior, reach 10 in vacuum-2During more than Pa, power transmission preheats, and treats that vacuum reaches 10 again-2Stop evacuation simultaneously after more than Pa It is filled with high-purity Ar, when Ar air pressure reaches -0.05MPa in stove, the power of smelting furnace is adjusted and carry out melting to monitor system, treat Stirring after raw material all melts carries out refine 3min, after refine, aluminium alloy is poured in water cooled copper mould, obtains Ce28Fe66.22Nb0.1Cu0.05B1.08Alloy cast ingot；
(3) alloy cast ingot coarse crushing is become the granule that particle diameter is 5～10mm, the ingot casting after then crushing is placed in vacuum electric In water jacketed copper crucible in arc quick quenching furnace, open electric arc and melt, after ingot casting melts completely, melt is passed through rotation molybdenum wheel and (turns Speed be 30m/s, piece footpath 250mm) cooling obtain nanocrystalline rapidly quenched magnetic powder Ce28Fe66.22Nb0.1Cu0.05B1.08；
(4) 100 eye mesh screens will be crossed after further for rapidly quenched magnetic powder ball mill crushing, then weigh 10g this magnetic powder 0.02g Graphene (Graphene parameter：The number of plies is 1～10 layer, and Graphene thickness is 0.8～20nm, and piece footpath is 50～1000nm) mix and put into vacuum Obtain after ball milling 3min in planetary ball mill tank mixing magnetic powder, after taking out mixing magnetic powder under Ar gas shielded, put into preprepared In mould, cold pressing under room temperature, pressure 700MPa 5 minutes and obtain finer and close isotropic magnet, then by gained isotropism Magnet utilizes discharging plasma sintering equipment in the way of adding copper sheathing thermal deformation (see Fig. 6), under 650 DEG C, pressure 50MPa, with The rate of deformation deformation 8min of 0.1mm/s, deflection 68%, obtain anisotropy nanocrystalline rare-earth permanent magnet, its magnetic property is such as Following table；
(5) 100 eye mesh screens will be crossed after further for rapidly quenched magnetic powder ball mill crushing, then weigh 10g this magnetic powder 0.02g Graphene (Graphene parameter：The number of plies is 1～10 layer, and Graphene thickness is 0.8～20nm, and piece footpath is 50～1000nm) mix and put into vacuum In planetary ball mill tank, ball milling 3min obtains mixing magnetic powder, takes out mixing magnetic powder, and put into preprepared under Ar gas shielded In hot pressing die, using induction heater, under 750 DEG C of temperature, pressure 200MPa, hot pressing obtains the isotropism of densification for 5 minutes Magnet, then by gained isotropic magnet in the way of adding copper sheathing thermal deformation (see Fig. 6), under 650 DEG C, pressure 100MPa, with The rate of deformation deformation 6min of 0.1mm/s, deflection 67.8%, obtain anisotropy nanocrystalline rare-earth permanent magnet, its magnetic property As following table：
Comparative example 5
In addition to without Graphene, according to method (+thermal deformation of colding pressing) same as Example 5, prepare Ce28Fe66.22Nb0.1Cu0.05B1.08Magnet.
Gained is not added with the magnetic property such as following table with the anisotropy nanocrystalline rare-earth permanent magnet of different Graphene additions：
Embodiment 6
(1) according to chemical formula Nd29.8Fe62.24Co6.76Zr0.1V0.1B1.0, the raw materials used rare earth for purity more than 99.5% Neodymium, the zirconium that purity is more than 99%, purity is 99.9% cobalt, and purity is 99.5% vanadium, the pure iron that purity is more than 99.9%, boron Content is the ferro-boron of 19.3wt%；
(2) by the Nd having configured29.8Fe62.24Co6.76Zr0.1V0.1B1.0Alloy raw material puts into intermediate frequency furnace melting rapid hardening In crucible, reach 10 in vacuum-2During more than Pa, power transmission preheats, and treats that vacuum reaches 10 again-2Stop after more than Pa taking out very Sky is simultaneously filled with high-purity Ar, adjusts the power of smelting furnace when Ar air pressure reaches -0.05MPa in stove and is melted to monitor system Refining, stirring after raw material all melts carries out refine 3min, after refine, aluminium alloy is poured in water cooled copper mould, obtains Nd29.8Fe62.24Co6.76Zr0.1V0.1B1.0Alloy cast ingot；
(3) alloy cast ingot coarse crushing is become the granule that particle diameter is 5～10mm, the ingot casting after then crushing is placed in vacuum electric In water jacketed copper crucible in arc quick quenching furnace, open electric arc and melt, after ingot casting melts completely, melt is passed through rotation molybdenum wheel and (turns Speed be 30m/s, piece footpath 250mm) cooling obtain nanocrystalline rapidly quenched magnetic powder Nd29.8Fe62.24Co6.76Zr0.1V0.1B1.0；
(4) 100 eye mesh screens will be crossed after further for rapidly quenched magnetic powder ball mill crushing, then weigh 10g this magnetic powder 0.02g Graphene Microplate (graphene microchip parameter：The number of plies is 10～100 layers, and thickness is 20～200nm, and piece footpath is 50～1000nm) mix and put into In vacuum planetary ball mill tank, ball milling 10min obtains mixing magnetic powder, takes out mixing magnetic powder and put into prior preparation under Ar gas shielded In good hot pressing die, using induction heater in 660 DEG C of temperature, hot pressing under pressure 200MPa obtains close to densification for 5 minutes Isotropic magnet, then by gained isotropic magnet with Free Transform mode (see Fig. 4), under 700 DEG C, pressure 80MPa, with The rate of deformation deformation 4min of 0.12mm/s, deflection 70%, obtain anisotropy nanocrystalline rare-earth permanent magnet.
Comparative example 6
In addition to without Graphene, according to method same as Example 6, prepare Nd29.8Fe62.24Co6.76Zr0.1V0.1B1.0Magnet.
Gained be not added with and different graphene microchip additions anisotropy nanocrystalline rare-earth permanent magnet magnetic property such as Following table：

Claims (7)

1. a kind of anisotropy nanocrystalline rare-earth permanent magnet is it is characterised in that this nanocrystalline rare-earth permanent magnet by chemical formula is REaFe100-a-b-cBbTMcNanocrystalline with Graphene and/or graphene microchip composition, wherein Graphene and/or graphene microchip Content be 0.01wt%～1wt%, described chemical formula REaFe100-a-b-cBbTMcIn, 28≤a≤33,0.9≤b≤1.35, 0.15≤c≤7, RE be Ce, Nd, Pr, Dy at least one, TM be Ga, Co, Cu, Nb, Al, Zr, V, Si, Ti at least A kind of.
2. the preparation method of anisotropy nanocrystalline rare-earth permanent magnet described in claim 1 is it is characterised in that processing step is as follows：
With REaFe100-a-b-cBbTMcMagnetic powder is raw material with Graphene or graphite microchip, the percent mass of Graphene or graphite microchip Number is 0.01%～1%, REaFe100-a-b-cBbTMcThe mass percent of magnetic powder is 99%～99.99%, by REaFe100-a-b- cBbTMcMagnetic powder mix homogeneously with Graphene or graphite microchip obtain mix magnetic powder, will mix magnetic powder room temperature, 100MPa～ 3～the 10min that colds pressing under 700MPa pressure obtains isotropism nanocrystalline magnet, or in 400 DEG C～750 DEG C of temperature, pressure Under 100MPa～700MPa, hot pressing 3～10min obtains isotropism nanocrystalline magnet；To cold pressing again or hot pressing gained isotropism Nanocrystalline magnet carries out thermal deformation 2min～8min under 650 DEG C～850 DEG C of temperature, pressure 50MPa～250MPa, obtain each to Different in nature nanocrystalline rare-earth permanent magnet.
3. according to claim 2 the preparation method of anisotropy nanocrystalline rare-earth permanent magnet it is characterised in that described graphite The structure level number of alkene is 1 layer～10 layers, and Graphene thickness is 0.8nm～20nm, and piece footpath is 50nm～1000nm.
4. according to claim 2 the preparation method of anisotropy nanocrystalline rare-earth permanent magnet it is characterised in that described graphite The structure level number of alkene microplate is 11 layers～100 layers, and thickness is 20nm～200nm, and piece footpath is 50nm～1000nm.
5. according to any claim in claim 2～4 anisotropy nanocrystalline rare-earth permanent magnet preparation method, its It is characterised by that described hot pressing, thermal deformation are to carry out using sensing heating or discharge plasma sintering mode, during using sensing heating, Hot pressing temperature is 550 DEG C～750 DEG C, hot pressing pressure is 100MPa～300MPa, and heat distortion temperature is 650 DEG C～850 DEG C, heat becomes Shape pressure is 100MPa～250MPa；During using discharge plasma sintering, hot pressing temperature is 400 DEG C～650 DEG C, hot pressing pressure is 200MPa～700MPa, heat distortion temperature is 650 DEG C～750 DEG C, thermal deformation pressure is 50MPa～200MPa.
6. according to any claim in claim 2～4 anisotropy nanocrystalline rare-earth permanent magnet preparation method, its Be characterised by thermal deformation speed be 0.1mm/s～0.5mm/s.
7. add the preparation method of the anisotropy nanocrystalline rare-earth permanent magnet of Graphene, its feature according to claim 5 Be thermal deformation speed be 0.1mm/s～0.5mm/s.
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CN107452456A (en) * 2017-08-29 2017-12-08 钢铁研究总院 A kind of high-intensity high-tenacity permanent magnet and preparation method thereof
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CN112670048A (en) * 2020-12-11 2021-04-16 东莞市嘉达磁电制品有限公司 Partial pressure sintering manufacturing method of neodymium iron boron magnet
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